CN106590624A - Light-emitting nano-particles and preparation method thereof - Google Patents
Light-emitting nano-particles and preparation method thereof Download PDFInfo
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- CN106590624A CN106590624A CN201611101035.XA CN201611101035A CN106590624A CN 106590624 A CN106590624 A CN 106590624A CN 201611101035 A CN201611101035 A CN 201611101035A CN 106590624 A CN106590624 A CN 106590624A
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- nano granule
- covering material
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/701—Chalcogenides
- C09K11/703—Chalcogenides with zinc or cadmium
Abstract
The invention discloses light-emitting nano-particles and a preparation method thereof. The light-emitting nano-particles have n layers of core-shell structures, including a light-emitting nano-particle core formed by a semiconductor material, an odd number of coating layers formed by a first coating material, and an even number of coating layers formed by a second coating material. The light-emitting nano-particles overcome the defects of lattice mismatch and built-in stress between a core material and a shell material in the prior art. The preparation method of the light-emitting nano-particles adopts a method for continuously growing the coating layers on surfaces of the light-emitting nano-particles, and is simple and feasible.
Description
Technical field
The present invention relates to lighting field, specifically a kind of luminous nano granule and preparation method thereof.
Background technology
At present, luminescent material is applied to into lighting field very common.Quantum dot (QD) is used as main Illuminant nanometer
Grain has had shown that the very high potentiality for being used for illumination application as phosphor material.
Quantum dot has in theory the stability of high-quantum efficiency and light conversion and energy transfer, but pure
Grain endures impact to the fullest extent because it is extremely sensitive on surface environment, often shows low quantum yield, and concentration quenching and thermal quenching.
In order to obtain high-quantum efficiency semiconductor-quantum-point and avoid concentration and temperature quenching, common scheme is to grow over the qds
Extra shell：The shell material with relatively wide quasiconductor energy gap is taken to realize the protection to core quantum dot and limit core
Quantum dot is stimulated the electronics of generation and hole is transferred to outside quantum dot, under many circumstances, it is necessary to keeping minimum
By shell oriented growth is to a certain thickness and forms a certain shape to keep optimum performance while lattice mismatch.But, due to
The reason for lattice mismatch and built-in stress between different core and shell material, extremely difficult synthetic method is needed to realize
Corresponding function.For example, the shell being made up of semi-conducting material ZnS is grown on the InP quantum dots as core.Here, ZnS makees
The defect of core InP quantum dot surfaces is strongly reduced for protective layer, and reduces concentration quenching.But, based on ZnS and
Lattice between InP is mismatched, very difficult more than the ZnS of 5 atomic layer level thickness in the growth of core InP quantum dot surfaces, with
The increase of ZnS thickness degree, cumulative stress is will appear from and quantum yield is declined.Another kind of method is handed in core InP quantum dot surfaces
For the shell material of growth ZnS and InP, by limiting each layer of thickness to overcome crystal in built-in stress.Meanwhile, InP-
Each layer of InP in ZnS multi-layer core-shell quanta point materials can carry out light conversion by light source activation, so as to improve the whole of quantum dot
Body light conversion efficiency.But, it is single because the photo and thermal stability of quantum dot is largely still determined by outermost material
The stability of multi-layer core-shell quantum dot itself is still quite limited.
The content of the invention
For the deficiencies in the prior art, the technical problem that the present invention is intended to solve be to provide a kind of luminous nano granule and its
Preparation method.The luminous nano granule is the luminous nano granule with n-layer nucleocapsid structure, including semi-conducting material is formed
The even number clad that the odd number clad and the second covering material that luminous nano granule core, the first covering material are formed is formed, gram
The defect of lattice mismatch in prior art between nuclear material and shell material and built-in stress is taken.
The present invention solves the problems, such as that the technical scheme of the material technology is to provide a kind of luminous nano granule, and its feature exists
In the luminous nano granule be the luminous nano granule with n-layer nucleocapsid structure, n >=2；Luminous nano granule includes half
What luminous nano granule core, the odd number clad of the first covering material formation and the second covering material that conductor material is formed was formed
Even number clad；
The composition of the composition, the composition of the first covering material and the second covering material of the luminous nano granule nuclear material
Molecular formula is M1x-M2y-M3z-A(X+2Y+3Z)/2；M1 is first selected from Li, Na, K, Rb, Cs, Be, Mg, Ca, Sr, Ba, Cu, Ag or Au
Element；M2 is selected from Cu, Ag, Au, Zn, Cd or Hg element；In elements or V A races of the M3 in B, Al, Ga, In, Tl, IV A races
Element；Elements or element in VII A race of the A in O, S, Se, Te, V A races；X=0-1 in molecular formula, y=0-1, z=0-1
And at least one of x, y and z value is more than 0；While the composition of luminous nano granule core and the odd number clad being adjacent
Composition between differ, differ between the composition of the composition of odd number clad and the even number clad being adjacent.
The present invention solves the technical scheme of the preparation method technical problem and is to provide a kind of preparation of luminous nano granule
Method, it is characterised in that comprise the following steps：
(1) it is luminous nano granule nuclear material, the first covering material presoma, excess surface active agent and excessive response is molten
Agent agitating heating 0.1-4h at 100-360 DEG C, the first covering material forerunner precursor reactant generates the first clad and grows into and sends out
Light nanoparticle core surface；
(2) by by the luminous nano granule of the first clad parcel, the second covering material presoma, excess surface activity
Agent and excessive response solvent agitating heating 0.1-4h at 100-360 DEG C, the second covering material forerunner precursor reactant generates second and wraps
Coating simultaneously grows into the first cover surface；
(3) by by the luminous nano granule of the second clad parcel, the first covering material presoma, excess surface activity
Agent and excessive response solvent agitating heating 0.1-4h at 100-360 DEG C, the first covering material forerunner precursor reactant generates three guarantees
Coating simultaneously grows into the second cover surface；
(4) by by the luminous nano granule of the 3rd clad parcel, the second covering material presoma, excess surface activity
Agent and excessive response solvent agitating heating 0.1-4h at 100-360 DEG C, the second covering material forerunner precursor reactant generates the 4th and wraps
Coating simultaneously grows into the 3rd cover surface；
(5) by that analogy, continued growth cladding, obtains the luminous nano granule of n-layer cladding；N >=2.
The surfactant is fatty acid, fatty amine, mercaptan or phosphide；
The first covering material presoma and the second covering material presoma are selected from inorganic acid salt, the metal of metallic element
The organometallic compound precursor of the acylate of element, the soap of metallic element or nonmetalloid；
The reaction dissolvent is water, polar organic solvent or non-polar organic solvent.
Compared with prior art, beneficial effect of the present invention is：Present invention growth cladding material on luminous nano granule core
Material, obtains high-quantum efficiency semiconductor light emitting nanoparticle core and avoids concentration and temperature quenching.Take with relatively
The covering material of wide quasiconductor energy gap realizes that the protection to luminous nano granule core and restriction luminous nano granule core are received
The electronics and hole for exciting generation is transferred to outside luminous nano granule core.On the one hand this structure improves the suction to exciting light
Receive, on the other hand limit inside excites the electronics of generation and the outside probability for shifting in hole, so as to improve Illuminant nanometer
The overall light conversion efficiency of granular core.
Description of the drawings
Fig. 1 is that a kind of luminous nano granule overall structure of embodiment of luminous nano granule of the present invention and preparation method thereof is shown
It is intended to；
Fig. 2 is that a kind of luminous nano granule overall structure of embodiment of luminous nano granule of the present invention and preparation method thereof is shown
It is intended to；(in figure：10th, luminous nano granule core；15th, the odd number clad that the first covering material is formed；25th, the second covering material
The even number clad of formation)
Specific embodiment
The specific embodiment of the present invention is given below.Specific embodiment is only used for further describing the present invention, does not limit
The application scope of the claims processed.
The invention provides a kind of luminous nano granule and preparation method thereof.
The luminous nano granule is the luminous nano granule with n-layer nucleocapsid structure, n >=2；Luminous nano granule
Luminous nano granule core 10, the cladding of odd number clad 15 and second of the first covering material formation formed including semi-conducting material
The even number clad 25 that material is formed.
The composition of the composition, the composition of the first covering material and the second covering material of the luminous nano granule nuclear material
Molecular formula is M1x-M2y-M3z-A(X+2Y+3Z)/2；M1 selected from Li, Na, K, Rb or Cs of I A races, Be, Mg, Ca, Sr of II A races or
Ba, Cu, Ag or Au of I B races；Cu, Ag or Au, Zn, Cd or the Hg of II B races of M2 selected from I B races；M3 selected from the B of III A races, Al,
Element in Ga, In or Tl, IV A, V A races；Elements of the A in V A races, O, S, Se or Te of VI A races, VII A races；X=0-
At least one of 1, y=0-1, z=0-1 and x, y and z value is more than 0；Simultaneously the composition of luminous nano granule core and with its phase
Differ between the composition of adjacent odd number clad, the composition of the composition of odd number clad and the even number clad being adjacent it
Between differ；
A kind of above-mentioned luminous nano granule, the M1 is Na, Li, Mg, Cu, Ag or Au.
A kind of above-mentioned luminous nano granule, the M2 is Zn or Cd.
A kind of above-mentioned luminous nano granule, the M3 is Ga, As, In or Tl.
A kind of above-mentioned luminous nano granule, the A is O, S, Se, As, P or Te.
The compound specifically CdS of the A of II B- VI, CdSe, CdTe, ZnS, ZnSe, ZnTe, HgS, HgSe, HgTe, CdSeS,
CdSeTe、CdSTe、ZnSeS、ZnSeTe、ZnSTe、HgSeS、HgSeTe、HgSTe、CdZnS、CdZnSe、CdZnTe、CdHgS、
CdHgSe、CdHgTe、HgZnS、HgZnSe、HggZnTe、CdZnSeS、CdZnSeTe、CdZnSTe、CdHgSeS、CdHgSeTe、
CdHgSTe, HgZnSeS, HgZnSeTe or HgZnSTe；
The compound specifically GaN of the A of III A- V, GaP, GaAs, AlN, AlP, AlAs, InN, InP, InAs, GaNP,
GaNAs、GaPAs、AlNP、AlNAs、AlPAs、InNP、InNAs、InPAs、GaAlNP、GaAlNAs、GaAlPAs、GaInNP、
GaInNAs, GaInPAs, InAlNP, InAlNAs or InAlPAs；
The compound specifically CuInS of the A of I B-, III A- VI2、CuInSe2、CuGaS2、CuGaSe2、AgInS2、AgInSe2、
AgGaS2And AgGaSe2；
The compound specifically LiAsSe of the A of I A-, V A- VI2、NaAsSe2Or KAsSe2。
The shape of luminous nano granule core 10, odd number clad 15 and even number clad 25 is in the luminous nano granule
Ball, cube, bar, silk, disk or many pods；For example, the CdS granules of rod-shape surround spherical CdSe granules.
Luminous nano granule 20 provides main application attribute, for example, launch wavelength and transmitting band；First covering material shape
Into the covering material of odd number clad 15 and second formed even number clad 25 formed luminous nano granule main body and shape.
First covering material and the second covering material have the attribute that strengthens luminous nano granule core or for whole luminous nano granule
Bring new attribute.It is substantially grown in Lattice Matching (preferably has on core<10%, preferably<5% lattice mismatch).
A kind of preparation method of above-mentioned luminous nano granule is as follows：
(1) it is luminous nano granule nuclear material, the first covering material presoma, excess surface active agent and excessive response is molten
Agent agitating heating 0.1-4h at 100-360 DEG C, the first covering material forerunner precursor reactant generates the first clad and grows into and sends out
Light nanoparticle core surface；
(2) by by the luminous nano granule of the first clad parcel, the second covering material presoma, excess surface activity
Agent and excessive response solvent agitating heating 0.1-4h at 100-360 DEG C, the second covering material forerunner precursor reactant generates second and wraps
Coating simultaneously grows into the first cover surface；
(3) by by the luminous nano granule of the second clad parcel, the first covering material presoma, excess surface activity
Agent and excessive response solvent agitating heating 0.1-4h at 100-360 DEG C, the first covering material forerunner precursor reactant generates three guarantees
Coating simultaneously grows into the second cover surface；
(4) by by the luminous nano granule of the 3rd clad parcel, the second covering material presoma, excess surface activity
Agent and excessive response solvent agitating heating 0.1-4h at 100-360 DEG C, the second covering material forerunner precursor reactant generates the 4th and wraps
Coating simultaneously grows into the 3rd cover surface；
(5) by that analogy, continued growth cladding, obtains the luminous nano granule of n-layer cladding；N >=2.
The surfactant is fatty acid (such as myristic acid, stearic acid, hexyl phosphoric acid), fatty amine (such as cetyl
Amine etc.), mercaptan (1- spicy thioalcohols etc.), phosphide (tri octyl phosphine, trioctylphosphine oxide (TOPO) etc.), and other are by physical absorption or change
Be bonded in one or more in the chemical molecular on luminous nano granule surface.
The first covering material presoma and the second covering material presoma are selected from the inorganic acid salt of metallic element (such as sulfur
Sour zinc, Caddy (Cleary)), acylate (such as zinc acetate, indium acetate), the soap of metallic element of metallic element is (such as stearic acid
Zinc, undecylenic acid cadmium) or nonmetalloid organometallic compound precursor (such as thiirane, tributyl selenium)；
The reaction dissolvent is water, polar organic solvent (such as chloroform, acrylate, trioctylphosphine oxide (TOPO) etc.) or nonpolar has
Machine solvent (such as octadecylene, octadecane hydrocarbon etc.).
Embodiment 1
A kind of structure of luminous nano granule is InP/ZnS/InP/ZnS.Luminous nano granule core 10 is InP, and first wraps
The odd number clad 15 for covering material formation is ZnS, and the even number clad 25 that the second covering material is formed is InP, anti-by repeating
InP/ZnS/InP/ZnS luminous nano granules should be synthesized.
Preparation method is：Octadecylene (ODE) is added to the concentration of 25 μm of ol/L after luminous nano granule core InP is washed
In, form solution A.In a nitrogen atmosphere, the thiirane of 2ml solution As, 0.5mmol trioctylphosphine oxide (TOPO)s, 1mmol is mixed into
Stir in the ODE of 10ml, obtain mixture A.Mixture A is slowly warmed up into 180 DEG C, and is kept for 30 minutes, reaction life
Into the first clad and grow into luminous nano granule core surface.By that analogy, second, third clad of continued growth.Closing
Into after, room temperature is cooled to, and alternately adopts ethanol and toluene to be precipitated to it and dissolved to clean impurity, finally given
InP/ZnS/InP/ZnS luminous nano granules.
First covering material ZnS and the second covering material InP are in the alternately parcel growth of luminous nano granule core InP surfaces.
First, by luminous nano granule core InP lattice-matched growths to the first covering material ZnS and the second covering material
In InP, the first covering material ZnS is strengthened the particular community of luminous nano granule core InP, while strengthening Illuminant nanometer
Granular core InP is to the absorption of exciting light and the efficiency of stimulated light emission.
Luminous nano granule core and the second covering material are commaterials, are all InP materials, and the first covering material is
ZnS.Therefore, for luminous nano granule core and the second covering material have theoretic high-quantum efficiency attribute and its
Light is overlapped or intersected.With luminous nano granule nuclear phase ratio, the first covering material is directed to a certain wavelength, for example, in ultraviolet and/or indigo plant
There is light absorbs attribute much better than in theory in color.
The present invention does not address part and is applied to prior art.
Claims (7)
1. a kind of luminous nano granule, it is characterised in that the luminous nano granule is the Illuminant nanometer with n-layer nucleocapsid structure
Granule, n >=2；Luminous nano granule includes that the luminous nano granule core of semi-conducting material formation, the first covering material are formed
Odd number clad and the second covering material formed even number clad；
The molecule of the composition of the composition, the composition of the first covering material and the second covering material of the luminous nano granule nuclear material
Formula is M1x-M2y-M3z-A(X+2Y+3Z)/2；M1 is selected from Li, Na, K, Rb, Cs, Be, Mg, Ca, Sr, Ba, Cu, Ag or Au element；M2
Selected from Cu, Ag, Au, Zn, Cd or Hg element；Elements or element in V A race of the M3 in B, Al, Ga, In, Tl, IV A races；A
Element or the element in VII A races in O, S, Se, Te, V A races；X=0-1 in molecular formula, y=0-1, z=0-1 and x, y and z
At least one of value be more than 0；Simultaneously the composition of the composition of luminous nano granule core and the odd number clad being adjacent it
Between differ, differ between the composition of the composition of odd number clad and the even number clad being adjacent.
2. luminous nano granule according to claim 1, it is characterised in that M1 is Na, Li, Mg, Cu, Ag or Au.
3. luminous nano granule according to claim 1, it is characterised in that M2 is Zn or Cd.
4. luminous nano granule according to claim 1, it is characterised in that M3 is Ga, As, In or Tl.
5. luminous nano granule according to claim 1, it is characterised in that A is O, S, Se, As, P or Te.
6. the preparation method of the luminous nano granule described in a kind of claim 1-5, it is characterised in that comprise the following steps：
（1）Luminous nano granule nuclear material, the first covering material presoma, excess surface active agent and excessive response solvent are existed
Agitating heating 0.1-4h at 100-360 DEG C, the first covering material forerunner precursor reactant generates the first clad and grows into luminous receiving
Rice grain core surface；
（2）By by the first clad parcel luminous nano granule, the second covering material presoma, excess surface active agent and
Excessive response solvent agitating heating 0.1-4h at 100-360 DEG C, the second covering material forerunner precursor reactant generates the second clad
And grow into the first cover surface；
（3）By by the second clad parcel luminous nano granule, the first covering material presoma, excess surface active agent and
Excessive response solvent agitating heating 0.1-4h at 100-360 DEG C, the first covering material forerunner precursor reactant generates the 3rd clad
And grow into the second cover surface；
（4）By by the 3rd clad parcel luminous nano granule, the second covering material presoma, excess surface active agent and
Excessive response solvent agitating heating 0.1-4h at 100-360 DEG C, the second covering material forerunner precursor reactant generates the 4th clad
And grow into the 3rd cover surface；
（5）By that analogy, continued growth cladding, obtains the luminous nano granule of n-layer cladding；N >=2；
The surfactant is fatty acid, fatty amine, mercaptan or phosphide；
The first covering material presoma and the second covering material presoma are selected from inorganic acid salt, the metallic element of metallic element
Acylate, the soap of metallic element or nonmetalloid organometallic compound precursor；
The reaction dissolvent is water, polar organic solvent or non-polar organic solvent.
7. the preparation method of luminous nano granule according to claim 6, it is characterised in that the surfactant is bean
At least one in cool acid, stearic acid, hexyl phosphoric acid, hexadecylamine, 1- spicy thioalcohols, tri octyl phosphine or trioctylphosphine oxide (TOPO)；
The first covering material presoma and the second covering material presoma are selected from zinc sulfate, Caddy (Cleary), zinc acetate, acetic acid
Indium, zinc stearate, undecylenic acid cadmium, thiirane or tributyl selenium；
The reaction dissolvent is at least one in water, chloroform, acrylate, trioctylphosphine oxide (TOPO), octadecylene or octadecane hydrocarbon.
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| CN107502337A (en) * | 2017-08-24 | 2017-12-22 | 南昌航空大学 | The preparation method of single-phase phosphor quantum dot and its White-light LED chip |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107502337A (en) * | 2017-08-24 | 2017-12-22 | 南昌航空大学 | The preparation method of single-phase phosphor quantum dot and its White-light LED chip |
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| CN113710615A (en) * | 2019-04-26 | 2021-11-26 | 信越化学工业株式会社 | Quantum dot, wavelength conversion material, backlight, image display device, and method for manufacturing quantum dot |
| CN112752828A (en) * | 2019-08-23 | 2021-05-04 | Ns材料株式会社 | Quantum dot and manufacturing method thereof |
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| US11795392B2 (en) * | 2020-04-20 | 2023-10-24 | Samsung Electronics Co., Ltd. | Cadmium-free quantum dot, quantum dot-polymer composite, and electronic device including the same |
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